2-(chloromethyl)-4,5-dihydro-1H-imidazole hydrochloride → 2-[(2-Imidazoline-2-ylmethyl)thio]-1H-naphth[2,3-d]imidazoldihydrochloride

HRID 2051775

반응식

HRID 2051775 반응식
[NH:1]1[C:5]2[CH:6]=[C:7]3[C:12](=[CH:13][C:4]=2[N:3]=[C:2]1[SH:14])[CH:11]=[CH:10][CH:9]=[CH:8]3.[ClH:15].[Cl:16][CH2:17][C:18]1[NH:19][CH2:20][CH2:21][N:22]=1>CN(C)C=O.C1(C)C=CC=CC=1>[ClH:16].[ClH:15].[NH:22]1[CH2:21][CH2:20][N:19]=[C:18]1[CH2:17][S:14][C:2]1[NH:3][C:4]2[CH:13]=[C:12]3[C:7](=[CH:6][C:5]=2[N:1]=1)[CH:8]=[CH:9][CH:10]=[CH:11]3

참가 물질

5

반응물 2

HCID 27609282-(chloromethyl)-4,5-dihydro-1H-imidazole hydrochlorideHCID 1785277551H-benzo[f]benzimidazole-2-thiol

생성물 1

HCID 705692132-[(2-Imidazoline-2-ylmethyl)thio]-1H-naphth[2,3-d]imidazoldihydrochloride수율 58.1%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6228Dimethylformamide용매

실험 절차

10.0 g of 1H-Naphth[2,3-d]imidazole-2-thiol and 8.0 g of 2-chloromethylimidazoline-hydrochloride were heated for 3 hours at 90° in 50 ml of dimethylformamide. The reaction mixture was cooled to room temperature and then diluted with 200 ml of toluene. The residue was suctioned filtered, washed well with toluene, and crystallised from 700 ml of methanol, with the addition of 300 ml of ether. 10.3 g of 2-[(2-Imidazoline-2-ylmethyl)thio]-1H-naphth[2,3-d]imidazol-dihydrochloride having an m.p. of 227°-228° were obtained.

후처리

  1. filtrationThe residue was suctioned filtered
  2. washwashed well with toluene
  3. customcrystallised from 700 ml of methanol, with the addition of 300 ml of ether

출처 및 근거

ORD 기록
ord-4c0801f701f74bbb9906b79febf8f3e0
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04182766

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